#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:40:51 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179802 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/98/7009870.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7009870
loop_
_publ_author_name
'Wietzke, Raphaël'
'Mazzanti, Marinella'
'Latour, Jean-Marc'
'Pécaut, Jacques'
_publ_section_title
;
 Solution and solid state structures of uranium(III) and lanthanum(III)
 iodide complexes of tetradentate tripodal neutral N-donor
 ligands †
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4167
_journal_paper_doi               10.1039/b004179n
_journal_year                    2000
_chemical_formula_sum            'C23 H23 I3 La N5'
_chemical_formula_weight         889.07
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.8260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7180(5)
_cell_length_b                   15.3889(8)
_cell_length_c                   9.9741(5)
_cell_measurement_temperature    143(2)
_cell_volume                     1342.64(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8639
_diffrn_reflns_theta_full        28.89
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    5.060
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    2.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         2.497
_refine_diff_density_min         -2.407
_refine_diff_density_rms         0.225
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6035
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0879P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                5890
_reflns_number_total             6035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004179n.txt
_cod_data_source_block           struc3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7009870
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La La 0.77299(4) 0.75358(2) -0.14709(3) 0.01642(9) Uani 1 1 d . . .
I1 I 0.84260(5) 0.58312(3) -0.30677(5) 0.02780(11) Uani 1 1 d . . .
I2 I 0.55776(5) 0.81470(3) 0.01884(5) 0.03037(12) Uani 1 1 d . . .
I3 I 1.10165(5) 0.80510(3) 0.11132(4) 0.02521(11) Uani 1 1 d . . .
N1 N 0.9089(6) 0.8041(4) -0.3162(6) 0.0194(10) Uani 1 1 d . . .
N2 N 0.7177(7) 0.9245(4) -0.1791(6) 0.0240(11) Uani 1 1 d . . .
N3 N 0.5034(6) 0.6741(4) -0.2927(6) 0.0228(11) Uani 1 1 d . . .
N4 N 0.5871(6) 0.8167(4) -0.4205(6) 0.0196(10) Uani 1 1 d . . .
N5 N 0.8143(7) 0.6246(4) 0.0534(7) 0.0258(12) Uani 1 1 d . . .
C1 C 0.6665(7) 0.8630(5) -0.4974(7) 0.0247(13) Uani 1 1 d . . .
H1A H 0.6702 0.9256 -0.4737 0.030 Uiso 1 1 calc R . .
H1B H 0.6050 0.8565 -0.6063 0.030 Uiso 1 1 calc R . .
C2 C 0.8260(8) 0.8323(5) -0.4579(8) 0.0231(13) Uani 1 1 d . . .
C3 C 0.8869(9) 0.8400(5) -0.5591(8) 0.0278(15) Uani 1 1 d . . .
H3 H 0.8259 0.8605 -0.6572 0.033 Uiso 1 1 calc R . .
C4 C 1.0397(8) 0.8173(6) -0.5151(8) 0.0306(15) Uani 1 1 d . . .
H4 H 1.0845 0.8230 -0.5823 0.037 Uiso 1 1 calc R . .
C5 C 1.1245(9) 0.7863(5) -0.3726(9) 0.0289(16) Uani 1 1 d . . .
H5 H 1.2284 0.7700 -0.3403 0.035 Uiso 1 1 calc R . .
C6 C 1.0551(8) 0.7797(5) -0.2778(8) 0.0262(14) Uani 1 1 d . . .
H6 H 1.1130 0.7568 -0.1808 0.031 Uiso 1 1 calc R . .
C7 C 0.4860(7) 0.8782(5) -0.3923(7) 0.0227(13) Uani 1 1 d . . .
H7A H 0.4244 0.8462 -0.3513 0.027 Uiso 1 1 calc R . .
H7B H 0.4148 0.9053 -0.4874 0.027 Uiso 1 1 calc R . .
C8 C 0.5765(8) 0.9479(4) -0.2847(7) 0.0213(12) Uani 1 1 d . . .
C9 C 0.5165(8) 1.0297(5) -0.2855(8) 0.0275(14) Uani 1 1 d . . .
H9 H 0.4184 1.0447 -0.3608 0.033 Uiso 1 1 calc R . .
C10 C 0.5993(9) 1.0893(5) -0.1770(9) 0.0308(15) Uani 1 1 d . . .
H10 H 0.5582 1.1451 -0.1753 0.037 Uiso 1 1 calc R . .
C11 C 0.7436(9) 1.0663(5) -0.0702(9) 0.0315(16) Uani 1 1 d . . .
H11 H 0.8030 1.1060 0.0061 0.038 Uiso 1 1 calc R . .
C12 C 0.7992(9) 0.9845(5) -0.0770(8) 0.0278(14) Uani 1 1 d . . .
H12 H 0.8997 0.9700 -0.0063 0.033 Uiso 1 1 calc R . .
C13 C 0.4976(7) 0.7423(5) -0.5168(7) 0.0219(12) Uani 1 1 d . . .
H13A H 0.5659 0.7075 -0.5460 0.026 Uiso 1 1 calc R . .
H13B H 0.4146 0.7659 -0.6089 0.026 Uiso 1 1 calc R . .
C14 C 0.4283(8) 0.6832(5) -0.4400(7) 0.0220(12) Uani 1 1 d . . .
C15 C 0.2956(8) 0.6376(5) -0.5244(8) 0.0278(15) Uani 1 1 d . . .
H15 H 0.2437 0.6457 -0.6291 0.033 Uiso 1 1 calc R . .
C16 C 0.2405(9) 0.5803(6) -0.4538(9) 0.0344(16) Uani 1 1 d . . .
H16 H 0.1505 0.5477 -0.5094 0.041 Uiso 1 1 calc R . .
C17 C 0.3179(8) 0.5707(6) -0.2998(9) 0.0320(16) Uani 1 1 d . . .
H17 H 0.2832 0.5311 -0.2481 0.038 Uiso 1 1 calc R . .
C18 C 0.4459(9) 0.6204(5) -0.2256(9) 0.0307(15) Uani 1 1 d . . .
H18 H 0.4966 0.6162 -0.1201 0.037 Uiso 1 1 calc R . .
C21 C 0.8473(8) 0.6535(5) 0.1926(8) 0.0268(14) Uani 1 1 d . . .
H21 H 0.8638 0.7140 0.2118 0.032 Uiso 1 1 calc R . .
C22 C 0.8583(9) 0.6001(6) 0.3080(8) 0.0313(16) Uani 1 1 d . . .
H22 H 0.8856 0.6228 0.4049 0.038 Uiso 1 1 calc R . .
C23 C 0.8284(9) 0.5124(6) 0.2785(8) 0.0324(16) Uani 1 1 d . . .
H23 H 0.8298 0.4740 0.3537 0.039 Uiso 1 1 calc R . .
C24 C 0.7966(10) 0.4818(6) 0.1381(9) 0.0357(17) Uani 1 1 d . . .
H24 H 0.7788 0.4216 0.1163 0.043 Uiso 1 1 calc R . .
C25 C 0.7906(8) 0.5392(5) 0.0292(8) 0.0262(14) Uani 1 1 d . . .
H25 H 0.7688 0.5171 -0.0669 0.031 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 La N3 115.29(17) . . ?
N1 La N2 76.56(19) . . ?
N3 La N2 106.63(19) . . ?
N1 La N4 63.69(16) . . ?
N3 La N4 63.37(18) . . ?
N2 La N4 61.10(18) . . ?
N1 La N5 136.16(19) . . ?
N3 La N5 82.04(19) . . ?
N2 La N5 139.69(19) . . ?
N4 La N5 145.18(18) . . ?
N1 La I3 80.93(11) . . ?
N3 La I3 161.03(13) . . ?
N2 La I3 86.03(12) . . ?
N4 La I3 135.50(12) . . ?
N5 La I3 79.25(13) . . ?
N1 La I1 70.34(13) . . ?
N3 La I1 74.46(13) . . ?
N2 La I1 143.07(13) . . ?
N4 La I1 89.20(13) . . ?
N5 La I1 77.20(14) . . ?
I3 La I1 104.081(15) . . ?
N1 La I2 145.58(13) . . ?
N3 La I2 73.68(13) . . ?
N2 La I2 69.11(13) . . ?
N4 La I2 96.40(12) . . ?
N5 La I2 76.31(14) . . ?
I3 La I2 98.766(15) . . ?
I1 La I2 140.796(17) . . ?
C6 N1 C2 117.1(6) . . ?
C6 N1 La 119.2(4) . . ?
C2 N1 La 121.2(4) . . ?
C12 N2 C8 117.7(6) . . ?
C12 N2 La 124.2(5) . . ?
C8 N2 La 115.7(4) . . ?
C18 N3 C14 118.2(6) . . ?
C18 N3 La 122.5(5) . . ?
C14 N3 La 119.1(5) . . ?
C7 N4 C1 109.2(6) . . ?
C7 N4 C13 111.2(5) . . ?
C1 N4 C13 108.7(5) . . ?
C7 N4 La 104.2(4) . . ?
C1 N4 La 115.0(4) . . ?
C13 N4 La 108.4(4) . . ?
C25 N5 C21 116.9(6) . . ?
C25 N5 La 128.7(5) . . ?
C21 N5 La 114.0(5) . . ?
N4 C1 C2 115.1(6) . . ?
N1 C2 C3 122.7(6) . . ?
N1 C2 C1 116.7(6) . . ?
C3 C2 C1 120.3(6) . . ?
C2 C3 C4 119.0(7) . . ?
C5 C4 C3 119.1(6) . . ?
C4 C5 C6 118.6(7) . . ?
N1 C6 C5 123.4(7) . . ?
N4 C7 C8 111.3(5) . . ?
N2 C8 C9 121.6(6) . . ?
N2 C8 C7 116.2(6) . . ?
C9 C8 C7 122.0(6) . . ?
C10 C9 C8 120.0(7) . . ?
C9 C10 C11 118.8(7) . . ?
C12 C11 C10 118.7(7) . . ?
N2 C12 C11 123.2(7) . . ?
N4 C13 C14 113.1(5) . . ?
N3 C14 C15 122.3(7) . . ?
N3 C14 C13 117.9(6) . . ?
C15 C14 C13 119.7(6) . . ?
C16 C15 C14 118.8(7) . . ?
C15 C16 C17 119.3(7) . . ?
C18 C17 C16 117.6(8) . . ?
N3 C18 C17 123.8(7) . . ?
N5 C21 C22 123.8(7) . . ?
C21 C22 C23 118.1(7) . . ?
C24 C23 C22 118.8(7) . . ?
C23 C24 C25 119.6(8) . . ?
N5 C25 C24 122.7(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La N1 2.670(5) . ?
La N3 2.675(6) . ?
La N2 2.676(6) . ?
La N4 2.712(5) . ?
La N5 2.720(6) . ?
La I3 3.2095(5) . ?
La I1 3.2885(6) . ?
La I2 3.3189(5) . ?
N1 C6 1.353(9) . ?
N1 C2 1.358(9) . ?
N2 C12 1.347(9) . ?
N2 C8 1.365(9) . ?
N3 C18 1.330(10) . ?
N3 C14 1.333(9) . ?
N4 C7 1.477(8) . ?
N4 C1 1.485(8) . ?
N4 C13 1.503(8) . ?
N5 C25 1.339(10) . ?
N5 C21 1.356(9) . ?
C1 C2 1.500(9) . ?
C2 C3 1.379(10) . ?
C3 C4 1.397(10) . ?
C4 C5 1.380(11) . ?
C5 C6 1.385(10) . ?
C7 C8 1.501(9) . ?
C8 C9 1.385(10) . ?
C9 C10 1.380(11) . ?
C10 C11 1.387(11) . ?
C11 C12 1.383(11) . ?
C13 C14 1.522(9) . ?
C14 C15 1.385(10) . ?
C15 C16 1.374(13) . ?
C16 C17 1.393(12) . ?
C17 C18 1.370(11) . ?
C21 C22 1.380(10) . ?
C22 C23 1.385(13) . ?
C23 C24 1.379(12) . ?
C24 C25 1.381(11) . ?
